摘要
建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS)快速检测茶叶中高氯酸盐的分析方法。样品经50%乙腈提取,石墨化炭黑(GCB)分散固相萃取净化,采用亲水作用色谱分离,在UPLC-MS/MS的多反应监测(MRM)模式下进行测定。对方法的提取和净化条件进行了系统优化,在优化好条件下,高氯酸盐在0.005~5.0 mg/kg浓度范围内呈现良好的二次曲线关系,相关系数(R^2)为0.9998,定量限为0.01 mg/kg。在4种添加浓度(0.005,0.05,0.1,1.0 mg/kg)下的加标回收率在75.2%~95.8%之间,日内和日间相对标准偏差小于10.2%,表明该方法具有很好的准确度和精密度。最后,将所建立的方法用于91个茶叶样品中高氯酸盐的分析,取得了较好的效果。
A method for the determination of perchlorate in tea by ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)was proposed.The sample was extracted with 50%acetonitrile aqueous solution,and then purified by graphitized carbon black(GCB)based dispersed solid phase extraction.Hydrophilic interaction chromatography(HILIC)-MS/MS in multiple reaction monitoring(MRM)mode was used to analyze perchlorate in tea.The experimental variables in sample preparation process were optimized.Under the optimal conditions,perchlorate showed a good relationship in the range of 0.005-1 mg/kg with R^20.9998.The recoveries of perchlorate spiked at four concentrations(0.005 mg/kg,0.05 mg/kg,0.1 mg/kg,1.0 mg/kg)were between 75.2%-95.8%with inter and intro-day relative standard deviations RSDs less than 10.2%,demonstrating good accuracy and precision of the proposed method.Finally,the proposed method was applied to risk monitoring of perchlorate in 90 tea samples.
作者
彭西甜
夏珍珍
胡西洲
郑丹
彭茂民
刘丽
张仙
夏虹
PENG Xitian;XIA Zhenzhen;HU Xizhou;ZHENG Dan;PENG Maomin;LIU Li;ZHANG Xian;XIA Hong(Institute of Agricultural Quality Standards and Testing Technology Research,Hubei Academy of Agricultural Science/Laboratory of Quality&Safety Risk Assessment for Agro-products(Wuhan),Ministry of Agriculture and Rural Affairs,Wuhan 430064)
出处
《分析科学学报》
CAS
CSCD
北大核心
2020年第2期275-279,共5页
Journal of Analytical Science
基金
国家自然科学基金(No.21607039)。
关键词
茶叶
高氯酸盐
超高效液相色谱-串联质谱
Perchlorate
Tea
Ultra-high performance liquid chromatography-tandem mass spectrometry
